CN105241849A - Spectral pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging method and Raman spectrum-mass spectrum microscopic imaging device - Google Patents
Spectral pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging method and Raman spectrum-mass spectrum microscopic imaging device Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0004—Imaging particle spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
- G01J3/4412—Scattering spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/443—Emission spectrometry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B21/00—Microscopes
- G02B21/0004—Microscopes specially adapted for specific applications
- G02B21/002—Scanning microscopes
- G02B21/0024—Confocal scanning microscopes (CSOMs) or confocal "macroscopes"; Accessories which are not restricted to use with CSOMs, e.g. sample holders
- G02B21/0032—Optical details of illumination, e.g. light-sources, pinholes, beam splitters, slits, fibers
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- G02B21/00—Microscopes
- G02B21/0004—Microscopes specially adapted for specific applications
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- G02B21/002—Scanning microscopes
- G02B21/0024—Confocal scanning microscopes (CSOMs) or confocal "macroscopes"; Accessories which are not restricted to use with CSOMs, e.g. sample holders
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- G02B21/0076—Optical details of the image generation arrangements using fluorescence or luminescence
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- G—PHYSICS
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- G02B21/002—Scanning microscopes
- G02B21/0024—Confocal scanning microscopes (CSOMs) or confocal "macroscopes"; Accessories which are not restricted to use with CSOMs, e.g. sample holders
- G02B21/008—Details of detection or image processing, including general computer control
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
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- G02B21/20—Binocular arrangements
Abstract
The invention relates to a spectral pupil laser differential confocal LIBS, a Raman spectrum-mass spectrum microscopic imaging method and a Raman spectrum-mass spectrum microscopic imaging device and belongs to the technical fields of confocal microscopic imaging, optical-spectrum imaging and mass spectrum imaging. In the invention, spectral pupil laser differential confocal imaging is combined with optical-spectrum and mass spectrum detection technologies, so that high-spatial-discrimination form imaging to a sample is carried out by means of a micro focus light spot of a spectral pupil laser differential confocal microscope which is subjected to ultra-discrimination technology treatment; mass spectrum detection to charged molecules and atoms in a micro zone of a sample is carried out by means of the mass spectrum detection system; micro zone optical spectrum detection is carried out to a focused light spot excitation spectrum (Raman spectrum, induced breakdown spectrum) of the spectral pupil laser differential confocal microscopic system through the optical-spectrum detection system; and high-spatial discrimination, high-sensitive imaging and high-sensitive detection to complete component information and form parameters of the sample micro zone is carried out through advantage complement and structural fusion of laser multi-spectrum detection. The invention provides a novel technical approach for imaging detection of substance components and formations in the field of biology, material and the like.
Description
Technical field
The invention belongs to confocal microscopic imaging technology, spectral imaging technology and mass spectrum imaging technical field, pupil differential confocal microscopic imaging technology, Laser-induced Breakdown Spectroscopy imaging technique, Raman spectrum imaging technology will be divided to combine with mass spectrum imaging technology, relate to a kind of point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method and device, have wide practical use in fields such as biology, material, mineral products, minute manufacturings.
Technical background
Mass spectrometer (MassSpectrometry) is ionized the component in sample, the charge atom of the different specific charges of generation, molecule or molecular fragment focused on respectively under the effect of Electric and magnetic fields and obtains the collection of illustrative plates instrument by the arrangement of mass-to-charge ratio size order.Mass spectrum imaging carries out mass spectrophotometry respectively to detect the distribution of specific mass-to-charge ratio (m/z) material to tiny area multiple in sample 2 dimensional region.
From the appearance of the substance assistant laser desorpted ionized this high sensitivity of the mid-80 in last century and high quality detection scope biological mass spectrometry imaging technique, open up field-biological mass spectrometry that mass-spectrometry one is brand-new, mass-spectrometric technique range of application is impelled to expand to the various fields of life science, the particularly application of mass spectrum in protein, nucleic acid, glycoprotein assay etc., not only for life science provides new tool, and also promote the development of mass-spectrometric technique self.
But there is following outstanding problem in existing substance assistant laser desorpted ionized mass spectrometer:
1) owing to utilizing simple Laser Focusing to carry out desorption ionization sample, thus still there is the problems such as Laser Focusing hot spot is large, mass spectrometry detection spatial resolution is not high in it;
2) cannot centering atom, molecule, intermediate ion and group etc. detect, its result constrains the accurate complete acquisition of sample component information;
3) mass spectrum imaging required time is long, and the relative sample of laser mass spectrometry instrument focal beam spot axial location often drifting problem occurs.
And " microcell " pattern of mineral products, space material and biological sample and the Obtaining Accurate of complete component information are all extremely important for scientific research and production testing.In fact, how detecting micro-area composition information is with sensitivity the important technological problems that the fields such as current mineral products analysis, biochemistry detection are urgently studied.
The intense pulse laser of Laser-induced Breakdown Spectroscopy focuses on sample surfaces can make sample ionization, excited sample can produce plasma, can obtain the atom of sample and Small molecular element forms information by the fail spectrum that gives off of detection energy of plasma; Utilize laser Raman spectroscopy technology can measure the molecule excitation spectrum of sample, obtain the chemical bond in sample and molecular structure information.Laser Raman spectroscopy technology, Laser-induced Breakdown Spectroscopy (LIBS) technology are combined and can to realize with mass spectrometry detection combine with technique having complementary advantages and structure function merges, utilize laser multispectral (mass spectrum, Raman spectrum and Laser-induced Breakdown Spectroscopy) integration technology to realize the complete component information detection of sample.
Pupil laser differential confocal technology is divided to utilize illumination to detect with detection light path non-co-line structure, not only significantly improve azimuthal resolution and the Focus accuracy of light path, realize the high-resolution imaging detection of sample topography, and can effectively suppress backscattering to disturb, improve spectrographic detection signal to noise ratio (S/N ratio).
Based on this, the present invention proposes a kind of point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method and device, its innovation is: a point pupil differential confocal microtechnic with high-space resolution ability merged mutually with laser Raman spectroscopy technology, Laser-induced Breakdown Spectroscopy (LIBS) technology and mass spectrometry detection technology first, can realize imaging and the detection of sample microcell high-space resolution and highly sensitive form and component.
The pattern component imaging detection that a kind of high-space resolution of the present invention confocal laser induced breakdown, Raman spectrum and mass spectrum micro imaging method and device can be the fields such as biology, material, physical chemistry, minute manufacturing provides a brand-new effective technical way.
Summary of the invention
The object of the invention is the spatial resolving power in order to improve mass spectrum imaging, suppressing the drift of focal beam spot relative sample in imaging process, a kind of point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method and device are proposed, to obtaining measurand micro-raman spectra information and component information simultaneously.Laser divides the detecting function of pupil differential confocal microscope focal beam spot to merge mutually with Laser Focusing desorption ionization function by the present invention, the small focal beam spot of point pupil differential confocal microscope through super resolution technology process is utilized to carry out the imaging of high-space resolution form to sample, Raman spectrum detection system is utilized to detect the Raman spectrum that point pupil confocal microscope system focal beam spot excited sample produces, utilize the charged molecule that mass spectrometry detection system produces point pupil differential confocal microscopic system focal beam spot desorption ionization sample, atoms etc. carry out microcell mass spectrum imaging, the plasma emission spectroscopy information utilizing Laser-induced Breakdown Spectroscopy detection system to produce point pupil differential confocal microscopic system focal beam spot desorption ionization sample carries out Laser-induced Breakdown Spectroscopy imaging, and then by sample composition information that fusion and the comparison of detection data information have obtained, then imaging and the detection of sample microcell high-space resolution and highly sensitive form and component is realized.
The object of the invention is to be achieved through the following technical solutions.
Of the present invention point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method, utilize high-space resolution to divide the focal beam spot of pupil differential confocal microscopic system to carry out axis to sample to focus and imaging, Raman spectrum detection system is utilized to detect the Raman spectrum that point pupil differential confocal microscopic system focal beam spot excited sample produces, utilize the charged molecule that mass spectrometry detection system produces point pupil differential confocal microscopic system focal beam spot desorption ionization sample, atoms etc. carry out microcell mass spectrum imaging, the plasma emission spectroscopy utilizing Laser-induced Breakdown Spectroscopy detection system to produce point pupil differential confocal microscopic system focal beam spot desorption ionization sample detects, and then imaging and the detection of sample microcell high-space resolution and highly sensitive form and component is then realized by the fusion of detection data information and compare of analysis, comprise the following steps:
Step one, the D type illumination iris that parallel beam is collected in mirror by the compression focal beam spot system of placing along incident light axis direction, the illumination of D type focus on sample;
Step 2, making computing machine control three-dimensional working platform drives sample to move up and down near D type illumination collection mirror foci along measuring surface normal direction, the D type along gathering optical axis direction placement is utilized to collect pupil, optical splitter, dichro iotac beam and the collection lens being positioned at dichro iotac beam reflection direction in spectrophotometric reflection direction, relaying amplifying lens detects with being positioned at relaying amplifying lens focal plane and carrying out segmentation about the first light intensity point probe and the second light intensity point probe that gather the placement of optical axis symmetry to amplification Airy, the strength characteristics obtaining Airy disk first microcell and Airy disk second microcell is respectively first from axle confocal axial strength curve and second from the confocal axial strength curve of axle,
Step 3, subtract each other process from axle confocal axial strength curve and second from the confocal axial strength curve of axle by first and obtain a point pupil differential confocal axial strength curve, utilize a point pupil differential confocal axial strength curve accurately can locate this axial height information of sample;
Step 4, computing machine are according to the null position z of point pupil differential confocal axial strength curve
avalue controls three-dimensional working platform and drives sample to move along measuring surface normal direction, and the focal beam spot making the illumination of D type collect mirror focuses on sample;
Step 5, utilize Raman spectrum detection system to detect the Raman spectrum collected through spectrophotometric reflection, dichro iotac beam transmission and spectral collection lens, record sample chemical key and the molecular structure information in corresponding focal beam spot region;
Step 6, change parallel beam light illumination mode, excite the microcell desorption ionization of sample to produce plasma plume;
Step 7, utilize ionized sample suction pipe to be produced by focal beam spot desorption ionization sample plasma plume in molecule, atom and ion suck in mass spectrometry detection system and carry out mass spectrum imaging, record the Information in Mass Spectra in corresponding focal beam spot region;
Step 8, utilize Laser-induced Breakdown Spectroscopy detection system to detect the Laser-induced Breakdown Spectroscopy of collecting through optical splitter transmission and Laser-induced Breakdown Spectroscopy collecting lens, record the sample element composition information in corresponding focal beam spot region;
The Information in Mass Spectra of the Laser Focusing microcell that the Raman spectral information of the Laser Focusing microcell that laser divides the pupil differential confocal Laser Focusing facula position height of specimen information that detection system records, laser Raman spectroscopy detection system to detect by step 9, computing machine, the Laser-induced Breakdown Spectroscopy information of the Laser Focusing microcell of Laser-induced Breakdown Spectroscopy detection system detection, mass spectrometry detection system record carries out fusion treatment, then obtains the height of focal beam spot microcell, spectrum and Information in Mass Spectra;
Step 10, computing machine control three-dimensional working platform makes the illumination of D type collect the next one region to be measured that mirror foci aims at sample, then operates by step 2 ~ step 9, obtains the height of next focal zone to be measured, spectrum and Information in Mass Spectra;
Step 11, repetition step 10, until all tested points on sample are all measured, then utilize computing machine to carry out process and can obtain sample shape information and complete component information.
Method of the present invention comprises can be makes parallel beam pass through to be shaped as annular beam after the vector beam generation systems, iris filter of the placement of incident light axis direction, and this annular beam is collected mirror through circular illumination again and focused on desorption ionization generation plasma plume on sample.
Method of the present invention comprises the illumination of D type and collects illumination collecting function that D type illumination iris and D type in mirror collect pupil and can collect circular illumination pupil and circular collection pupil in mirror by circular illumination and come.
High-space resolution laser of the present invention divides pupil differential confocal induced breakdown, Raman spectrum-spectrum-mass spectrum microscopic imaging device, comprise pointolite, the collimation lens placed along incident light axis direction, compression focal beam spot system and focal beam spot to sample D type illumination collection mirror D type illumination iris, pupil collected by the D type comprised along gathering the D type illumination collection mirror that optical axis direction is placed, optical splitter and the dichro iotac beam being positioned at spectrophotometric reflection direction, be positioned at the collection lens of dichro iotac beam reflection direction, relaying amplifying lens and be positioned at relaying amplifying lens focal plane and about optical axis symmetry place the first light intensity point probe and the second light intensity point probe, also comprise and be positioned at dichro iotac beam transmission direction for detecting the Raman collection lens of Raman spectrum and being positioned at the Raman spectrum detection system of Raman collection lens focus, be positioned at optical splitter transmission direction for the Laser-induced Breakdown Spectroscopy collecting lens of exploring laser light induced breakdown spectroscopy and Laser-induced Breakdown Spectroscopy detection system, and ionized sample suction pipe and the mass spectrometry detection system of the ion body feathers component of mirror focal beam spot desorption ionization is collected for the illumination of D type, incident light axis and the angle gathered between optical axis are 2 α, and symmetrical about measuring surface normal.
Apparatus of the present invention comprise compression focal beam spot system and can substitute with the vector beam generation systems of the generation vector beam placed along incident light axis direction and iris filter.
Apparatus of the present invention comprise D type illumination collection mirror and can be replaced circular illumination collection mirror.
Apparatus of the present invention comprise the first light intensity point probe and the second light intensity point probe can substitute with a ccd detector.
Beneficial effect
The present invention contrasts prior art, has the following advantages:
1) a point pupil differential confocal microtechnic with high-space resolution ability is merged mutually with mass spectrometry detection technology, make a point hot spot for pupil differential confocal microscopic imaging system realize focusing-detection and sample desorption ionization dual-use function, sample microcell mass spectrographic high spatial mass spectrum micro-imaging can be realized;
2) in conjunction with the detection of Raman spectrum and Laser-induced Breakdown Spectroscopy, overcome existing laser mass spectrometry instrument and centering atom, molecule, intermediate ion and group etc. cannot carry out the deficiency that detects, the mutual supplement with each other's advantages and the structure function that realize laser multispectral (mass spectrum, Raman spectrum and Laser-induced Breakdown Spectroscopy) component imaging detection merge, and can obtain microcell component information more comprehensively;
3) utilize the zero crossing of point pupil differential confocal curve to carry out sample to focus in advance, minimum focal beam spot is made to focus on sample surfaces, sample microcell high-space resolution mass spectrometry detection and microcell micro-imaging can be realized, effectively play the potential differentiated between point pupil differential confocal system altitude;
4) utilize a point pupil differential confocal curve zero crossing to carry out sample and focus process in advance, existing mass spectrometer can be suppressed because of the drifting problem of the relative sample of focal beam spot in long-time mass spectrum imaging;
5) utilize compression focal beam spot technology, improve the spatial resolving power of laser mass spectrometry instrument;
6) utilize a point pupil structured light bundle oblique incidence sounding, overcome the defect that existing confocal microscopic imaging technology cannot suppress focal plane interference of stray light, anti-parasitic light ability is strong.
Accompanying drawing explanation
Fig. 1 is point pupil laser differential confocal LIBS, a Raman spectrum-mass spectrum micro imaging method schematic diagram;
Fig. 2 is point pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method and the installation drawing of embodiment 1;
Fig. 3 is point pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method and the installation drawing of embodiment 2;
Wherein: 1-pointolite, 2-collimation lens, 3-parallel beam, 4-compresses focal beam spot system, mirror is collected in the illumination of 5-D type, 6-D type illumination iris, pupil collected by 7-D type, 8-incident light axis, 9-sample, 10-measuring surface normal, 11-plasma plume, 12-gathers optical axis, 13-gathers lens, 14-relaying amplifying lens, 15-focal plane, 16-amplifies Airy disk, 17-first light intensity point probe, 18-second light intensity point probe, 19-Airy disk first microcell, 20-Airy disk second microcell, 21-first is from the confocal axial strength curve of axle, 22-second is from the confocal axial strength curve of axle, 23-differential confocal axial strength curve, 24-computing machine, 25-three-dimensional working platform, 26-ionized sample suction pipe, 27-mass spectrometry detection system, 28-optical splitter, 29-Laser-induced Breakdown Spectroscopy collecting lens, 30-Laser-induced Breakdown Spectroscopy detection system, 31-vector beam generation systems, 32-iris filter, 33-circular illumination collects mirror, 34-circular illumination pupil, 35-circular collection pupil, 36-CCD detector, 37-outgoing beam attenuator, 38-detecting light beam attenuator, 39-pulsed laser, 40-collector lens, 41-Optic transmission fiber, 42-Laser-induced Breakdown Spectroscopy, 43-dichro iotac beam, 44-Raman spectrum, 45-Raman spectral collection lens, 46-Raman spectrum detection system.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
As shown in Figure 1, wherein, the ring light transverse super-resolution system that the D type illumination iris 6 throwing light on collection mirror 5 by compression focal beam spot system 4 and D type is formed, for compressing focal beam spot lateral dimension for core methed of the present invention.
Following examples all realize on Fig. 1 basis.
Embodiment 1
In point pupil laser differential confocal LIBS as shown in Figure 2, Raman spectrum-mass spectrum microscopic imaging device, compression focal beam spot system 4 is substituted by vector beam generation systems 31, iris filter 32, D type illumination collection mirror 5 can be collected mirror 33 by circular illumination and substitute, and the first hot spot detector 17 and the second hot spot detector 18 are substituted by ccd detector 36.
Point pupil laser differential confocal LIBS as shown in Figure 2, Raman spectrum-mass spectrum microscopic imaging device comprises pointolite 1, the collimation lens 2 placed along incident light axis 8 direction, vector beam generation systems 31, iris filter 32 and focal beam spot collect the circular illumination pupil 34 of mirror 33 to the circular illumination of sample 9, also comprise the circular collection pupil 35 that circular illumination collects mirror 33, be positioned at the optical splitter 28 gathering optical axis 12 direction, be positioned at the dichro iotac beam 43 of optical splitter 28 reflection direction and be positioned at the collection lens 13 of dichro iotac beam 43 reflection direction, relaying amplifying lens 14 and the ccd detector 36 be positioned on relaying amplifying lens 14 focal plane 15, and the ionized sample suction pipe 26 of ion body feathers 11 component and the mass spectrometry detection system 27 of mirror 33 focal beam spot desorption ionization is collected for circular illumination, incident light axis 8 and the angle gathered between optical axis 12 are 2 α, and it is symmetrical about measuring surface normal 10.
The function of main composition is as follows:
The laser focusing system that the circular illumination pupil 34 collecting mirror 33 to the circular illumination of sample 9 by pointolite 1, the collimation lens 2 placed along incident light axis 8, vector beam generation systems 31, iris filter 32, focal beam spot is formed is for generation of the small focal beam spot exceeding diffraction limit, and this super diffraction microsize hot spot has the dual-use function measured sample surfaces and produce surface plasma.
By collect along the circular illumination gathering optical axis 12 direction the circular collection pupil 35 of mirror 33, optical splitter 28, be positioned at optical splitter 28 reflection direction dichro iotac beam 43 and be positioned at the collection lens 13 of dichro iotac beam 43 reflection direction, relaying amplifying lens 14, be positioned at laser that the ccd detector 36 on relaying amplifying lens 14 focal plane 15 forms and divide pupil differential confocal detection system to carry out precision to sample 9 to focus, and the facula position that mirror 33 focuses on sample 9 is collected to circular illumination carry out axial location, record the height of specimen of corresponding focal beam spot position;
By the Raman spectrum detection system of collecting the circular collection pupil 35 of mirror 33, optical splitter 28, the dichro iotac beam 43 being positioned at optical splitter 28 reflected light direction and Raman collection lens 45 and the Raman spectrum detection system 46 that is positioned at Raman spectral collection lens 45 focus place along the circular illumination gathering optical axis 12 direction and forming, for detecting the Raman spectrum 44 of sample 9, record sample molecule structure and the chemical bond information in corresponding focal beam spot region;
The mass spectrometry detection system be made up of ionized sample suction pipe 26 and mass spectrometry detection system 27 detects charge atom, molecule etc. in plasma plume 11 based on time-of-flight method (TOF), carry out flight time mass spectrum detection.
The Laser-induced Breakdown Spectroscopy detection system that the collection lens 13 placed by edge collection optical axis 12, optical splitter 28, the Laser-induced Breakdown Spectroscopy collecting lens 29 being positioned at optical splitter 28 transmitted light direction and the spectrum investigating system 30 being positioned at Laser-induced Breakdown Spectroscopy collecting lens 29 focus place are formed, for detecting the Laser-induced Breakdown Spectroscopy 42 of sample 9, record the sample element composition information in corresponding focal beam spot region;
The tight focusing system of radial polarisation light longitudinal field that the circular illumination pupil 34 collecting mirror 33 by vector beam generation systems 31, iris filter 32 and circular illumination is formed is for compressing focal beam spot lateral dimension.
The three-dimensional motion system be made up of computing machine 24, three-dimensional working platform 25 can be carried out axis to sample 9 and be focused location and 3-D scanning.
The process of sample being carried out to high resolution mass spectrum imaging mainly comprises the following steps:
The light beam of step one, pointolite 1 outgoing collimates as parallel beam 3 after collimation lens 2, this parallel beam 3 generates annular beam through vector beam generation systems 31, iris filter 32, and this annular beam is focused to through the circular illumination pupil 34 of circular illumination collection mirror 33 small spot exceeding diffraction limit again and is radiated on sample 9;
Step 2, utilize computing machine 24 to control three-dimensional working platform 25 to make by circular collection pupil 35, relaying amplifying lens 14 and be positioned at the laser that the ccd detector 36 on relaying amplifying lens 14 focal plane 15 forms and divide pupil differential confocal detection system to carry out axial scan to sample 9, carry out segmentation to amplification Airy disk 16 to detect, the strength characteristics obtaining Airy disk first microcell 19 and Airy disk second microcell 20 is respectively first from axle confocal axial strength curve 21 and second from the confocal axial strength curve 22 of axle;
Step 3, subtract each other process from axle confocal axial strength curve 21 and second from the confocal axial strength curve 22 of axle by first and obtain a point pupil differential confocal axial strength curve 23, utilize a point pupil differential confocal axial strength curve 23 accurately can locate this axial height information of sample 9;
Step 4, computing machine 24 are according to the null position z of point pupil differential confocal axial strength curve 23
avalue controls three-dimensional working platform 25 and drives sample 9 to move along measuring surface normal 10 direction, and the focal beam spot making circular illumination collect mirror 33 focuses on sample 9, realizes initially focusing sample 9;
Step 5, utilize Raman spectrum detection system 46 to reflecting through optical splitter 28, Raman spectrum 44 that dichro iotac beam 43 transmission and Raman spectral collection lens 45 are collected detects, and records sample chemical key and the molecular structure information in corresponding focal beam spot region;
Step 6, change pointolite 1 mode of operation, improve illumination intensity, excites the microcell desorption ionization of sample 9 to produce plasma plume 11;
Step 7, utilize ionized sample suction pipe 26 to be produced by focal beam spot desorption ionization sample 9 plasma plume 11 in molecule, atom and ion suck in mass spectrometry detection system 27 and carry out mass spectrum imaging, record the Information in Mass Spectra in corresponding focal beam spot region;
Step 8, utilize Laser-induced Breakdown Spectroscopy detection system 30 to detect the Laser-induced Breakdown Spectroscopy 42 of collecting through optical splitter 28 transmission and Laser-induced Breakdown Spectroscopy collecting lens 29, record the sample element composition information in corresponding focal beam spot region;
The Information in Mass Spectra of the Laser Focusing microcell that the Raman spectrum 44 of the Laser Focusing microcell that laser is divided the pupil confocal detection Laser Focusing microcell shape information that system records by step 9, computing machine 24, Raman spectrum detection system 46 detects, the Laser-induced Breakdown Spectroscopy information of Laser-induced Breakdown Spectroscopy detection system 30 exploring laser light focusing microcell, mass spectrometry detection system 27 record carries out fusion treatment, obtains the height of focal beam spot microcell, spectrum and Information in Mass Spectra;
Step 10, computing machine 24 control three-dimensional working platform 24 makes circular illumination collection mirror 33 aim at the next one region to be measured of sample, then operates by step 2 ~ step 9, obtains the height of next focal zone to be measured, spectrum and Information in Mass Spectra;
Step 11, repetition step 10, until all tested points on sample 9 are all measured, then utilize computing machine 18 to carry out data fusion and image reconstruction process, can obtain sample shape information and complete component information.
Embodiment 2
In point pupil laser differential confocal LIBS as shown in Figure 3, Raman spectrum-mass spectrum microscopic imaging device, pointolite 1 is substituted by the Optic transmission fiber 41 of pulsed laser 39, collector lens 40, collector lens 40 focus, the illumination of D type is collected mirror 5 and is substituted by circular illumination collection mirror 33, and the first hot spot detector 17 and the second hot spot detector 18 are substituted by ccd detector 36.Meanwhile, in laser focusing system, introduce outgoing beam attenuator 37, divide in pupil differential confocal detection system at laser and introduce detecting light beam attenuator 38.
Light intensity regulating system is formed, for the spot intensity of decay focal beam spot and ccd detector 36 detection, with light intensity demand during location, accommodate sample surface by outgoing beam attenuator 37 and detecting light beam attenuator 38.
The process of sample being carried out to high resolution mass spectrum imaging mainly comprises the following steps:
Step 2 in embodiment 1, utilizing computing machine 24 to control three-dimensional working platform 25 makes by circular collection pupil 35, the laser that relaying amplifying lens 14 is formed with the ccd detector 36 be positioned on relaying amplifying lens 14 focal plane 15 divides pupil differential confocal detection system to carry out axial scan to sample 9, segmentation detection is carried out to amplification Airy disk 16, the strength characteristics obtaining Airy disk first microcell 19 and Airy disk second microcell 20 is respectively first from axle confocal axial strength curve 21 and second from the confocal axial strength curve 22 of axle, regulate detecting light beam attenuator 38, for decaying, light intensity detects to avoid ccd detector 36 supersaturation,
Step 6 is pulsed laser 39 mode of operation for a change, adjusts irradiating light beam attenuator 37 to strengthen the focal beam spot intensity that circular illumination collects mirror 33, excites the microcell desorption ionization of sample 9 to produce plasma plume 11;
All the other formation methods are identical with embodiment 1 with process.
Below by reference to the accompanying drawings the specific embodiment of the present invention is described, but these explanations can not be understood to limit scope of the present invention.
Protection scope of the present invention is limited by the claims of enclosing, and any change on the claims in the present invention basis is all protection scope of the present invention.
Claims (7)
1. one kind of point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method, it is characterized in that: utilize high-space resolution to divide the focal beam spot of pupil differential confocal microscopic system to carry out axis to sample and focus and imaging, Raman spectrum detection system is utilized to detect the Raman spectrum that point pupil differential confocal microscopic system focal beam spot excited sample produces, utilize the charged molecule that mass spectrometry detection system produces point pupil differential confocal microscopic system focal beam spot desorption ionization sample, atoms etc. carry out microcell mass spectrum imaging, the plasma emission spectroscopy utilizing Laser-induced Breakdown Spectroscopy detection system to produce point pupil differential confocal microscopic system focal beam spot desorption ionization sample detects, and then imaging and the detection of sample microcell high-space resolution and highly sensitive form and component is then realized by the fusion of detection data information and compare of analysis, comprise the following steps:
The D type illumination iris (6) that step one, the compression focal beam spot system (4) making parallel beam (3) pass through to place along incident light axis (8) direction, the illumination of D type are collected in mirror (5) focuses on sample (9);
Step 2, making computing machine (24) control three-dimensional working platform (25) drives sample (9) to move up and down along measuring surface normal (10) direction at D type illumination collection mirror (5) near focal point, utilize and collect pupil (7) along gathering the D type placed in optical axis (12) direction, optical splitter (28), the dichro iotac beam (43) of optical splitter (28) reflection direction and be positioned at the collection lens (13) of dichro iotac beam (43) reflection direction, relaying amplifying lens (14) and be positioned at relaying amplifying lens (14) focal plane (15) and about gather optical axis (12) symmetry place the first light intensity point probe (17) and the second light intensity point probe (18) to amplification Airy (16) carry out segmentation detect, the strength characteristics obtaining Airy disk first microcell (19) and Airy disk second microcell (20) is respectively first from axle confocal axial strength curve (21) and second from the confocal axial strength curve (22) of axle,
Step 3, subtract each other process from axle confocal axial strength curve (21) and second from the confocal axial strength curve (22) of axle by first and obtain point pupil differential confocal axial strength curve (23), utilize point pupil differential confocal axial strength curve (23) accurately can locate this axial height information of sample (8);
Step 4, computing machine (24) are according to the null position z of point pupil differential confocal axial strength curve (23)
avalue controls three-dimensional working platform (25) and drives sample (9) along the motion of measuring surface normal (10) direction, and the focal beam spot making the illumination of D type collect mirror (5) focuses on sample (9);
Step 5, utilize Raman spectrum detection system (46) to detect the Raman spectrum (44) collected through optical splitter (28) reflection, dichro iotac beam (43) transmission and spectral collection lens (45), record sample chemical key and the molecular structure information in corresponding focal beam spot region;
Step 6, change parallel beam (3) light illumination mode, excite the microcell desorption ionization of sample (8) to produce plasma plume (9);
Step 7, utilize ionized sample suction pipe (26) to be produced by focal beam spot desorption ionization sample (9) plasma plume (11) in molecule, atom and ion suck in mass spectrometry detection system (27) and carry out mass spectrum imaging, record the Information in Mass Spectra in corresponding focal beam spot region;
Step 8, utilize Laser-induced Breakdown Spectroscopy detection system (30) to detect the Laser-induced Breakdown Spectroscopy (42) of collecting through optical splitter (28) transmission and Laser-induced Breakdown Spectroscopy collecting lens (29), record the sample element composition information in corresponding focal beam spot region;
The Information in Mass Spectra of the Laser Focusing microcell that the Laser-induced Breakdown Spectroscopy (42) of the Laser Focusing microcell that the Raman spectrum (37) of the Laser Focusing microcell that laser is divided the pupil differential confocal Laser Focusing facula position height of specimen information that detection system records by step 9, computing machine (24), laser Raman spectroscopy detection system (39) detects, Laser-induced Breakdown Spectroscopy detection system (30) detect, mass spectrometry detection system (27) record carries out fusion treatment, then obtains height and the Information in Mass Spectra of focal beam spot microcell;
Step 10, computing machine (24) control three-dimensional working platform (25) makes the illumination of D type collect the next one region to be measured that mirror (5) focus aims at sample (9), then operate by step 2 ~ step 9, obtain the height of next focal zone to be measured, spectrum and Information in Mass Spectra;
Step 11, repetition step 10, until all tested points on sample (9) are all measured, then utilize computing machine (24) to carry out process and can obtain sample shape information and complete component information.
2. one according to claim 1 divides pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method, it is characterized in that: comprise step one and can be and make parallel beam (3) be shaped as annular beam by vector beam generation systems (31), the iris filter placed along incident light axis (8) direction after (32), this annular beam is collected mirror (33) through circular illumination again and is focused on the upper desorption ionization of sample (9) and produce plasma plume (11).
3. one according to claim 1 divides pupil laser differential confocal LIBS, Raman spectrum-mass spectrum micro imaging method, it is characterized in that: comprise the illumination of D type and collect illumination collecting function that D type illumination iris (6) and D type in mirror (5) collect pupil (7) and can collect the middle circular illumination pupil (34) of mirror (33) by circular illumination and circular collection pupil (35) has come.
4. one kind of point of pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging device, it is characterized in that: comprise pointolite (1), the collimation lens (2) placed along incident light axis (8) direction, compression focal beam spot system (4) and focal beam spot to sample (9) D type throw light on collection mirror (5) D type illumination iris (6), pupil (7) collected by the D type comprised along gathering D type illumination collection mirror (5) placed in optical axis (12) direction, optical splitter (28) and be positioned at the dichro iotac beam (43) of optical splitter (28) reflection direction, be positioned at the collection lens (13) of dichro iotac beam (43) reflection direction, relaying amplifying lens (14) and be positioned at relaying amplifying lens (14) focal plane (15) and about optical axis symmetry place the first light intensity point probe (17) and the second light intensity point probe (18), also comprise and be positioned at dichro iotac beam (43) transmission direction for detecting the Raman collection lens (45) of Raman spectrum (44) and being positioned at the Raman spectrum detection system (46) of Raman collection lens (45) focus, be positioned at Laser-induced Breakdown Spectroscopy collecting lens (29) and Laser-induced Breakdown Spectroscopy detection system (30) that optical splitter (28) transmission direction is used for exploring laser light induced breakdown spectroscopy (42), and ionized sample suction pipe (26) and the mass spectrometry detection system (27) of ion body feathers (11) component of mirror (5) focal beam spot desorption ionization is collected for the illumination of D type, incident light axis (8) and the angle gathered between optical axis (12) are 2 α, and symmetrical about measuring surface normal (10).
5. one according to claim 4 divides pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging device, it is characterized in that: comprising compression focal beam spot system (4) can substitute with the vector beam generation systems (31) of the generation vector beam placed along incident light axis (8) direction and iris filter (32).
6. one according to claim 4 divides pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging device, it is characterized in that: comprise D type illumination collection mirror (5) and can be replaced circular illumination collection mirror (33).
7. one according to claim 4 divides pupil laser differential confocal LIBS, Raman spectrum-mass spectrum microscopic imaging device, it is characterized in that: comprising the first light intensity point probe (17) and the second light intensity point probe (18) can substitute with a ccd detector (36).
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| US15/208,633 US20170018415A1 (en) | 2015-07-17 | 2016-07-13 | Divided-aperture laser differential confocal libs and raman spectrum-mass spectrum microscopic imaging method and device |
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